NMR spectrometer and method of NMR measurement

Abstract

There is disclosed a microchip reactor-type apparatus for effecting organic synthesis and reactions. The apparatus can be used in combination with many analytical instruments. The apparatus has a magnet for producing a static magnetic field for NMR measurements, a sample tube placed within the static magnetic field and holding a deuterated solvent therein, and a microchip reactor inserted inside the sample tube. A sample solution to be investigated is introduced into the channel formed in the microchip reactor while the microchip reactor is inserted inside the sample tube holding the deuterated solvent therein.

1. An NMR spectrometer having a magnet for producing a static magnetic field for NMR measurements, a sample tube placed within the static magnetic field produced by the magnet and holding a deuterated solvent therein, and a microchip reactor inserted inside the sample tube,
 wherein said microchip reactor includes an introduction portion for introducing plural reagents from plural channels and a reaction portion disconnectably connected with the introduction portion and acting to cause a reagent or a reaction liquid introduced from the introduction portion to mix and react with another reagent, 
 wherein said introduction portion has an introduction channel for introducing a reagent introduced from the outside into the reaction portion and a discharge channel for permitting the reaction liquid discharged from the reaction portion to be discharged to the outside, and 
 wherein said reaction portion has (i) a reaction channel in communication with the introduction channel and acting to cause plural reagents pumped from the introduction channel to be mixed and reacted with each other and (ii) a discharge passage for connecting the reaction channel and the discharge channel with each other to return the reaction liquid produced in the reaction channel to the introduction portion. 
 
     
     
       2. An NMR spectrometer as set forth in  claim 1 , wherein said introduction portion is a microchip reactor having a substrate of a chemically-resistant resin and a microchannel formed in the substrate. 
     
     
       3. An NMR spectrometer as set forth in  claim 1  or  2 , wherein inlet holes for introducing reagents and a discharge hole for discharging a reaction liquid are formed in the same side surface of said introduction portion. 
     
     
       4. An NMR spectrometer as set forth in  claim 1 , wherein said reaction portion is a microchip reactor having a substrate of glass or quartz and a microchannel formed in the substrate. 
     
     
       5. A method of NMR measurement implemented by an NMR spectrometer having a magnet for producing a static magnetic field for NMR measurements, a sample tube placed in a vertical bore formed in the magnet and holding a deuterated solvent therein, and a microchip reactor inserted inside the sample tube, said method of NMR measurement consisting of introducing a sample solution to be investigated into channels in the microchip reactor while the microchip reactor is inserted inside the sample tube holding the deuterated solvent therein. 
     
     
       6. A method of NMR measurement as set forth in  claim 5 , wherein said sample solution is measured by NMR spectroscopy while stopping flow of the sample solution. 
     
     
       7. A method of NMR measurement as set forth in  claim 5 , wherein said sample solution is measured by NMR spectroscopy without stopping flow of the sample solution. 
     
     
       8. A method of NMR measurement as set forth in any one of  claims 5  to  7 , wherein said sample solution is delivered from a syringe pump or pipette. 
     
     
       9. A method of NMR measurement as set forth in  claim 8 , wherein said sample solution is forcibly injected by a manual injector into flow of the solvent delivered by a syringe pump, HPLC pump, or pipette. 
     
     
       10. A method of NMR measurement as set forth in any one of  claims 5  to  7 , wherein said sample solution is delivered by an HPLC autosampler. 
     
     
       11. A method of NMR measurement as set forth in  claim 10 , wherein said sample solution is forcibly injected by the HPLC autosampler into flow of a solvent delivered by an HPLC pump.